HRID637763

反应详情

EQUATION

反应方程式

HRID 637763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

40 g (0.24 mol) of 2-mercaptobenzothiazole (MBT), 4 mg (0.02×10-3 mol) of copper (II) acetate, (Cu(OAc)2. H2O), 4.08 g (0.24 mol) of ammonia, and 120 g of isopropanol are placed in a glass autoclave equipped with a jacket for the circulation of a heating liquid, a thermometer, a pressure measuring device and a stirring device. The reaction mixture is heated to 70° C., stirred vigorously, and placed under an oxygen pressure of 4 bar. Absorption of oxygen is noted immediately and a precipitate, dibenzothiazyl disulfide (MBTS), is formed. After 6.5 hours the reaction is discontinued and the precipitate is filtered off, washed with isopropanol, and dried under a vacuum at 50° C. 37.8 g of a product are obtained in this manner. Upon elementary analysis, IR, NMR and MS, the product formed is found to correspond to dibenzothiazyl disulfide. The purity is found to be 100% upon chromatographic analysis (melting point 178° C.).

WORKUP

后处理

  1. customequipped with a jacket for the circulation of a heating liquid
  2. customAbsorption of oxygen